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GB/T 6609.1-2018: Chemical analysis methods and determination of physical performance of alumina -- Part 1: Determination of trace elements content -- Inductively coupled plasma atomic emission spectrometry method Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid GB/T 6609.1: Historical versions
Similar standardsGB/T 6609.1-2018: Chemical analysis methods and determination of physical performance of alumina -- Part 1: Determination of trace elements content -- Inductively coupled plasma atomic emission spectrometry method---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT6609.1-2018 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 71.100.10 H 12 Chemical analysis methods and determination of physical performance of alumina - Part 1.Determination of trace elements content - Inductively coupled plasma atomic emission spectrometry method Issued on: MAY 14, 2018 Implemented on: FEBRUARY 01, 2019 Issued by. State Administration for Market Regulation; Standardization Administration of the People's Republic of China. Table of ContentsForeword... 3 1 Scope... 6 2 Method summary... 6 3 Reagents... 7 4 Instruments... 8 5 Specimens... 8 6 Analysis steps... 8 7 Calculation of analysis results... 11 8 Precision... 11 9 Quality assurance and control... 12 10 Test report... 12 Annex A (normative) Preparation of standard stock solutions... 14 Annex B (normative) PTFE sealed sample analyzer... 17 Chemical analysis methods and determination of physical performance of alumina - Part 1.Determination of trace elements content - Inductively coupled plasma atomic emission spectrometry method1 ScopeThis Part of GB/T 6609 specifies the method for the determination of trace element content in metallurgical grade alumina (expressed as oxides. Na2O, K2O, Fe2O3, CuO, MgO, CaO, ZnO, V2O5, TiO2, Ga2O3, MnO, Li2O, BeO, Cr2O3, B2O3). This Part applies to the determination of trace element content in metallurgical grade alumina. The determination range is shown in Table 1.2 Method summaryPlace the test material in a polytetrafluoroethylene-sealed dissolver. Dissolve it in hydrochloric acid at a constant temperature (dissolution method I), or place the test material in a microwave digestion system and digest it with sulfuric acid at high temperature and high pressure (dissolution method II). Introduce the test solution into an inductively coupled plasma spectrometer. Excite it with an argon plasma light source and measure the spectrum. Correct for matrix effects on the measurement using the matrix matching method.3 ReagentsUnless otherwise stated, only confirmed guaranteed reagents and grade 1 water are used in the analyses. 3.1 Sulfuric acid (1+1). 3.2 Hydrochloric acid (1+1). 3.3 Sulfuric acid (1+2). 3.4 Hydrochloric acid (3+1). 3.5 Aluminum, w (Al) ≥99.999%. Pre-wash with a small amount of concentrated nitric acid, then wash with water to remove the nitric acid, rinse twice with anhydrous ethanol or acetone, and dry. 3.6 Alumina matrix solution (20 mg/mL). 3.6.1 Matrix Solution I. Weigh 5.288 g of aluminum (3.5) into a 1000 mL beaker. Cover with a watch glass. Add 300 mL of hydrochloric acid (3.2) in portions. After the violent reaction subsides, slowly heat until completely dissolved. Add a few drops of hydrogen peroxide (ρ = 1.10 g/mL). Boil for several minutes. Cool. Transfer the solution to a 500 mL volumetric flask. Dilute to the mark with water. Shake well. Store in a polyethylene bottle. 3.6.2 Matrix Solution II. Weigh 5.288 g of aluminum (3.5) into a 1000 mL beaker. Cover with a watch glass. Add 330 mL of sulfuric acid (3.1) in portions. Slowly heat until completely dissolved. Cool. Transfer the solution to a 500 mL volumetric flask. Dilute to the mark with water. Shake well. Store in a polyethylene bottle.4 Instruments4.1 Inductively coupled plasma atomic emission spectrometer. 4.2 Microwave digester. 4.3 Polytetrafluoroethylene sealed sample dissolver. See Annex B for a diagram of the device. 4.4 Oven. rated temperature is not less than 350°C, temperature control accuracy is ±3°C. 4.5 Desiccant. use new activated alumina as the desiccant.5 Specimens5.1 The specimens should be able to pass through a 0.125 mm standard sieve. 5.2 The specimen is dried in an oven (4.4) at 300°C ± 3°C for 2 h and then placed in a desiccator (4.5) to cool to room temperature.6 Analysis steps6.1 Test material Weigh the specimens (5) according to Table 2 to the nearest 0.0001 g. 6.2 Number of determinations The determinations are performed twice independently. Take the average value. 6.3 Blank test Carry out a blank test along with the test material (6.1). 6.4 Preparation of analytical solution 6.4.1 Sample dissolution method I Weigh the test material (6.1) according to Table 2 and place it in a 100 mL polytetrafluoroethylene reaction cup. Add 10 mL of hydrochloric acid (3.4). Cover the polytetrafluoroethylene reaction cup. Place in a polytetrafluoroethylene sealed sample dissolver (4.3). Place in an oven (4.4). Insulate at 240°C ± 3°C for 5 h. Remove. Cool to room temperature. Transfer the solution to a volumetric flask of the corresponding volume as shown in Table 2.Rinse the reaction cup with water. Combine the wash solution in the volumetric flask. Dilute to the mark with water. Mix thoroughly. 6.4.2 Sample dissolution method II Weigh the test material (6.1) according to Table 2 and place it in a 100 mL microwave digestion reaction cup. Add 10 mL of sulfuric acid (3.3). Cover the reaction cup lid and place it in the microwave digestion apparatus. Dissolve under the selected microwave digestion optimal measurement procedure. After the test material is completely dissolved, cool it to room temperature. Transfer into a 100 mL volumetric flask. Wash the reaction cup with water. Wash the liquid into a volumetric flask. Dilute with water to the mark. Mix well. This method is not applicable for the determination of CaO content. 6.5 Preparation of series standard solutions 6.5.1 Sample dissolution method I According to the amount of alumina in the test solution, transfer an appropriate amount of aluminum matrix solution (3.6.1) into a set of 100 mL volumetric flasks, so that the amount of alumina in the standard solution is basically the same as that in the test solution. According to the mass fraction of each element in the sample, add an appropriate amount of standard solution (3.8.1) or (3.8.2) of the element to be tested, so that the type and acidity of the acid in the standard solution are basically the same as those in the test solution. Dilute with water to the mark. Mix well. Store in polyethylene bottles. Use the test solution without standard solution as the blank solution, so that the content of the tested element should be within the range of the working curve. The number of standard solutions in the series shall not be less than 5.The mass fractions of each element should be distributed as evenly as possible. 6.5.2 Sample dissolution method II According to the amount of alumina in the test solution, transfer an appropriate amount of aluminum matrix solution (3.6.2) into a set of 100 mL volumetric flasks, so that the amount of alumina in the standard solution is basically the same as that in the test solution. According to the mass fraction of each element in the sample, add an appropriate amount of standard solution (3.8.1) or (3.8.2) of the element to be tested, so that the type and acidity of the acid in the standard solution are basically the same as those in the test solution. Dilute with water to the mark. Mix well and store in a polyethylene bottle. Use the test solution without standard solution as the blank solution, ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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